WO2015193156A1 - Synthetic diamond optical elements - Google Patents
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- WO2015193156A1 WO2015193156A1 PCT/EP2015/062971 EP2015062971W WO2015193156A1 WO 2015193156 A1 WO2015193156 A1 WO 2015193156A1 EP 2015062971 W EP2015062971 W EP 2015062971W WO 2015193156 A1 WO2015193156 A1 WO 2015193156A1
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/02—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3083—Birefringent or phase retarding elements
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/32—Holograms used as optical elements
Definitions
- the present invention relates to synthetic diamond optical elements. Certain embodiments relate to the provision of an alternative to synthetic diamond optical elements comprising thin film anti-reflective coatings. Particular embodiments relate to synthetic diamond optical elements having optical, thermal, and mechanical characteristics suitable for high power optical applications although synthetic diamond optical elements as described herein may be used in other applications where the provision of an antireflective coating is undesirable due to factors including mechanical robustness, chemical inertness, low absorbance, and high thermal conductivity. Certain further embodiments relate to the provision of birefringent diamond optical elements having these characteristics.
- Standard thin film anti-reflective coatings on synthetic diamond optical elements have excellent performance in terms of minimising reflection, but are limited in high power optical systems due to the ease with which they are damaged. Due to high absorbance and/or poor thermal conductivity the anti-reflective coating tends to be the weak point in any synthetic diamond window resulting in a synthetic diamond window with a low laser induced damage threshold (LIDT). Furthermore, even if the absorption level of a thin film anti-reflective coating is relatively low, the thin film can still fail in high power density optical applications. For example, for a 20 kW infrared laser system damage of thin film anti-reflective coatings is problematic and current thin film anti-reflective coating solutions are unlikely to be compatible with laser systems operating at 40 kW or more.
- LIDT laser induced damage threshold
- Such high power laser systems are desirable for a number of applications including laser produced plasma (LPP) extreme ultraviolet (EUV) lithography systems to drive integrated circuit processing to smaller dimensions.
- LPP laser produced plasma
- EUV extreme ultraviolet
- Such extreme optical applications will require a synthetic diamond window capable of handling extreme power densities and this will require the combination of: (1) a synthetic diamond material with the required dimensions and desired bulk optical characteristics including low optical reflectance/absorption/scatter; and; (2) an anti-reflective surface finish capable of handling extreme power densities.
- Thin film anti-reflective coatings can also be problematic in terms of their mechanical integrity, e.g. if subjected to scratching or abrasion.
- anti-reflective surface patterns such as moth-eye structures can be formed directly in the surface of an optical window material in order to provide an anti-reflective surface finish without the requirement of a coating. While such anti-reflective surface patterns have been successfully fabricated in a range of optical window materials, the application of this technology to synthetic diamond windows has proved problematic.
- the anti-reflective performance of such surface finishes has been variable due to the difficulty in processing precisely defined surface patterns into diamond material because of the extreme hardness, low toughness, and chemical inertness of diamond materials.
- Surface processing of poly crystalline diamond materials is further complicated by the fact that they comprise diamond grains having different orientations and different processing rates.
- This surface and subsurface damage in the synthetic diamond window causes a number of inter-related detrimental effects including: (1) a reduction in the laser induced damage threshold of the synthetic diamond window; (2) a reduction in the power at which the synthetic diamond window can operate; and (3) a reduction in the optical performance of the synthetic diamond window as a result of beam aberrations caused by the surface and sub-surface damage.
- a moth eye surface structure can be formed directly in diamond material to reduce reflection.
- a surface structure can be fabricated by first etching a reverse moth eye structure into silicon by lithographic techniques and then growing diamond material on the etched surface by chemical vapour deposition. The silicon is then dissolved to leave the diamond material with a moth eye structure.
- a multi-layer structure including an outer diamond layer with a flat outer surface has a reflectance of about 18% at a wavelength of 10 ⁇ , the reflectance being dominated by single-surface reflectance from the front face of the outer diamond layer (15%).
- reflectance is reduced to 7% at a wavelength of 10 ⁇ .
- US5334342 discloses a similar method of fabricating moth-eye surface structures in diamond material by patterning a reverse moth eye structure into a substrate, growing diamond material on the patterned substrate, and then removing the substrate to leave the diamond material with a moth eye surface structure.
- J. F. DeNatale et al [Fabrication and characterization of diamond moth eye antireflective surfaces on Germanium, J. Appl. Phys. 71, 1388 (1992)] have disclosed a similar approach by patterning a germanium substrate with a surface relief (moth eye) structure and then overgrowing a thin diamond film on the patterned substrate such that the thin diamond film retains the underlying surface structure of the patterned substrate. It is described that the progressive gradation in the effective refractive index between air and the composite substrate has reduced Fresnel reflection losses to below 1%. This provides a means of overcoming the high refractive index and surface roughness considerations that often limit optical applications of polycrystalline diamond thin films.
- T.V. Kononenko Formation of antireflective surface structures on diamond films by laser patterning, Applied Physics A, January 1999, Volume 68, Issue 1, pp 99-102 discloses an alternative to the substrate patterning and diamond over-growth technique disclosed in the previously described prior art.
- This paper describes diamond surface microstructuring by a laser ablation technique. The optical transmission of the diamond films was found to increase from 70% to 80% at a wavelength of 10.6 ⁇ by forming a microstructured surface by laser ablation.
- the transmittance value of 80% is still rather low and this would indicate that the quality of the diamond material is relatively poor, the surface structures fabricated in the diamond windows are not precisely defined, or that significant surface or sub-surface damage has been introduced into the diamond crystal structure when forming anti-reflective surface micro-structures.
- the paper does not indicate how the anti-reflective surface structures were fabricated in the diamond windows.
- Previously described methods of fabricating anti-reflective surface structures in diamond windows have involved either substrate patterning and diamond overgrowth or direct patterning via laser ablation. An alternative technique is to directly etch anti-reflective surface structures into diamond windows.
- the Uppsala group have indicated that diamond-based optics provide an attractive alternative for high-power laser optics due to their damage resistance, reduced thermal lensing, and transparency from the UV to the far-IR spectral regions.
- the Uppsala group have highlighted the need for better surface patterning for diamond-based optics and have proposed an inductively coupled plasma etching approach which involves patterning a resist layer on an optical-quality synthetic diamond using direct-write electron-beam lithography followed by dry etching in an inductively coupled plasma (ICP).
- ICP inductively coupled plasma
- the gases used for the diamond etching are 0 2 and Ar and a typical ICP etch recipe is disclosed as comprising: gas flows of 7 seem (standard cubic centimeters per minute) of 0 2 , and 8 seem of Ar; a chamber pressure of 2.5 mTorr; an ICP power of 600 W; bias voltages varied between -100 and -180 V; and sample etch times of between 2 and 20 minutes.
- a synthetic diamond optical element comprising an anti-reflective surface pattern formed directly in the surface of the synthetic diamond material and which has low absorbance and low reflectance while also having low surface and sub-surface crystal damage thus exhibiting a high laser induced damage threshold. It is a further aim to develop a technique for fabricating such anti-reflective surface patterns in diamond material which is relatively quick, low cost, and within acceptable processing errors.
- the aforementioned background information relates to the provision of a synthetic diamond optical element comprising an anti-reflective surface pattern formed directly in the surface of the synthetic diamond material.
- a synthetic diamond optical element comprising an anti-reflective surface pattern formed directly in the surface of the synthetic diamond material.
- quarter and half wave plates are essential optical components in many applications and allow for the polarization of incident light to be manipulated.
- Current waveplate technology suffers from various limitations including waveplate size and laser induced damage threshold (LIDT).
- LIDT laser induced damage threshold
- LIDT laser induced damage threshold
- laser induced damage can be especially problematic. This is because zero order waveplates are typically made from two pieces of birefringent material cemented together at a particular orientation relative to one another. This thin cement layer typically absorbs more laser energy than the birefringent material and can cause heating problems.
- birefringent surface patterns can be formed directly in the surface of an optical window material in order to provide a birefringent surface finish without the requirement of a separate coating material. While such birefringent surface patterns have been successfully fabricated in a range of optical window materials, the application of this technology to synthetic diamond windows has proved problematic for the same reasons as outlined above for antireflective surface patterns.
- the present applicant's earlier patent application PCT/EP2014/054183 describes an inductively coupled plasma reactive ion etching (ICP RIE) process for fabricating an anti- reflective surface pattern directly in the surface of a synthetic diamond material which has low absorbance and low reflectance while also having low surface and sub-surface crystal damage thus exhibiting a high laser induced damage threshold.
- ICP RIE inductively coupled plasma reactive ion etching
- the moth-eye surface will begin to act as a diffraction grating and light will be lost from the zeroeth grating order to additional transmitted and reflected grating orders.
- the ideal structure periodicity is determined by the largest value at which additional, non-zeroeth, grating orders are suppressed.
- the optical surface pattern should have a fill fraction within a defined range, the fill fraction defined as [area of projection in one periodic unit]/[area of the periodic unit].
- This area based 2-dimension fill fraction parameter has been found to be important to functional performance and is distinct from a 1 -dimensional fill factor parameter defined as [width of projection]/[length of periodic unit].
- a 1 -dimensional fill factor parameter defined as [width of projection]/[length of periodic unit].
- an optical element comprising: synthetic diamond material; and an optical surface pattern formed directly in at least one surface of the synthetic diamond material, wherein the optical surface pattern comprises a plurality of projections separated by trenches, the projections spaced apart with a periodicity d, wherein the periodicity d is between 65 and 99% of a zeroeth order diffraction limit above which non zeroeth diffraction orders are observed at an operating wavelength ⁇ , wherein the optical surface pattern has a fill fraction in a range 0.1 to 0.6, the fill fraction defined as [area of projection in one periodic unit]/[area of the periodic unit], and wherein the optical element has an absorption coefficient measured at room temperature of ⁇ 0.2 cm "1 at a wavelength of 10.6 ⁇ .
- the optical surface pattern may be configured with trenches having a depth-to-width aspect ratio in a range 1.2 to 3 (although a wider range of 0.8 to 3 may be applicable for certain antireflective surface patterns).
- a lower depth-to -width ratio has been found to be more readily fabricating into diamond materials in a more precise manner but if the depth-to -width ratio is too low then non-zero grating orders can become visible with increasing structure periodicity.
- an optical system comprising: an optical element as defined above; and a light source configured to generate light at a power of at least 300 W, 500 W, 1 kW, 3 kW, 5 kW, 10 kW, 15 kW, 20 kW, 25 kW, 30 kW, 35 kW, 40 kW, 45 kW, or 50 kW and transmit said light through the optical element.
- Figure 1 shows a schematic flow diagram of a method of fabricating an optical element comprising synthetic diamond material with an optical surface finish pattern formed directly in a surface of the synthetic diamond material;
- Figure 2 shows a schematic illustration of a portion of an anti-reflective pattern in a surface of a synthetic diamond optical element indicating depth, width, and periodicity dimensional parameters
- Figure 3 shows a schematic illustration of anti-reflective surface patterns having cylindrical and square projections indicating that anti-reflective surface patterns comprising square projections have a wider etched area and a lower depth-to-width aspect ratio;
- Figure 4 shows a graph illustrating how reflectivity at 10.6 ⁇ changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising cylindrical projections with a periodicity of 2.12 ⁇ and a depth of 1.72 ⁇ ;
- Figure 5 shows a graph illustrating how reflectivity at 10.6 ⁇ changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising square projections with a periodicity of 2 ⁇ and a depth of 1.72 ⁇ ;
- Figure 6 shows a graph illustrating how reflectivity at 10.6 ⁇ changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising square projections with a periodicity of 4 ⁇ and a depth of 1.72 ⁇ ;
- Figure 7 shows a schematic illustration in plan view of a portion of a birefringent pattern in a surface of a synthetic diamond optical element, the birefringent pattern comprising an elongate projection with elongate trenches disposed either side of the elongate projection;
- Figure 8 shows a schematic illustration in cross-sectional view of a birefringent surface pattern having elongate projections which has a trapezoidal cross-sectional shape
- Figure 9 shows a graph illustrating how transmission changes with line width and etch depth at an operating wavelength of 10.6 ⁇ for a birefringent surface pattern as illustrated in Figure 8 with a periodicity of 4 ⁇ and a sidewall taper angle of 5°;
- Figure 10 shows a schematic diagram of a high power laser system comprising a high power laser source and an optical element formed of synthetic diamond material with an optical surface pattern formed directly in a surface of the synthetic diamond material.
- NV " defect has an electronic spin which can be manipulated to function as a quantum bit or alternatively as a quantum sensing element.
- the NV " defect can be optically excited, manipulated using microwaves, and emits fluorescent light which is characteristic of its electronic spin state.
- the NV " electronic spin defect should have a long quantum coherence time and this requires the NV " electronic spin defect to be located in a highly pure diamond lattice environment which has a low concentration of crystal defects and low internal stress which can otherwise detrimentally reduce the quantum coherence time of the NV " electronic spin defects disposed within the diamond crystal lattice.
- Another requirement for quantum sensing and quantum information processing applications is that the fluorescent light emitted from the NV " electronic spin defects needs to be efficiently out-coupled from the diamond material to a suitable processor or detector configuration and in this regard it is desirable to fabricate nanowires, optical waveguide structures, and photonic cavity structures into the diamond material in order to effectively out-couple photons emitted from the NV " electronic spin defects.
- Inductively coupled plasma etching similar to that used by Uppsala University and discussed previously in the background section of this specification
- fabrication processes tend to introduce surface and sub-surface damage into the diamond crystal structure which adversely effects the quantum coherence time of the near-surface NV " electronic spin defects coupled to the optical surface structures.
- Groups developing structures for diamond quantum devices have experimented with a variety of different combinations of gas flow rates, ICP powers, and pressures for fabricating optical out-coupling structures in single crystal CVD diamond material without introducing significant quantities of surface and sub-surface damage into the diamond crystal structure.
- ICP RIE inductively coupled plasma reactive ion etching
- an oxygen etchant which has an oxygen gas flow of between 30 to 50 seem 0 2 , a chamber pressure of approximately 10 mTorr, and an ICP power of approximately 700 W. It is reported that this etch recipe allows the formation of very well defined surface structures while avoiding the formation of etch grass between the desired surface structures.
- the shape and quantity of the etched optical structures in a diamond surface can be controlled by varying the ICP power during the etching process.
- ICP power for example, in the fabrication of nano-wires in the surface of single crystal CVD diamond material a multi-step ICP RIE process is reported including applying an ICP power of 700 W for two minutes, an ICP power of 600 W for three minutes, and an ICP power of 1000 W for five minutes.
- etch masks are reported in the diamond quantum device literature including A1 2 0 3 particles, Au particles, Si0 2 particles, evaporated Au, and FOx e-beam resist.
- the present applicant has realized that the requirements for out-coupling structures such as nanowires, optical waveguide structures, and photonic cavity structures in quantum sensing and quantum information processing applications are very similar to the requirements for the fabrication of better anti-reflective surface patterns in transmissive diamond windows suitable for high power laser applications. That is, the etching technology developed for quantum sensing and quantum information processing applications can be transferred into the field of transmissive optics to provide a synthetic diamond window for high power laser applications comprising an anti-reflective surface pattern, such as a moth-eye pattern, formed directly in the surface of the synthetic diamond window and which has low reflectance and high transmittance while also having low surface and sub-surface crystal damage thus exhibiting a high laser induced damage threshold.
- an anti-reflective surface pattern such as a moth-eye pattern
- the etching technology developed for quantum sensing and quantum information processing applications is utilized for etching nanowires, optical waveguide structures, and photonic cavity structures in single crystal CVD diamond material comprising fluorescent NV " defects
- the etching technology is applied to low absorbance optical quality diamond material, such as high quality poly crystalline CVD diamond material, to fabricate low surface damage anti-reflective surface finishes, such as moth-eye structures, therein and thus produce optical elements having a combination of low absorbance, low reflectance, and a high laser induced damage threshold.
- a method of fabricating an optical element comprises: forming a patterned resist layer 2 on at least one surface of a synthetic diamond material 4; etching 3 the at least one surface of the synthetic diamond material 4 through the patterned resist layer 2; and removing the patterned resist layer to leave an anti-reflective surface pattern 6 formed directly in the at least one surface of the synthetic diamond material 4, wherein the etching comprises, for example, an inductively coupled plasma reactive ion etching (ICP RIE) process comprising an oxygen gas flow rate of between 20 to 50 seem 0 2 , a chamber pressure of between 5 and 20 mTorr, and an ICP power of between 600 and 1100 W.
- ICP RIE inductively coupled plasma reactive ion etching
- the inductively coupled plasma reactive ion etching process comprises one or more of: an oxygen flow rate between 25 and 35 seem 0 2; a chamber pressure between 7 and 15 mTorr; and an ICP power between 700 and 1000 W.
- the inductively coupled plasma reactive ion etching process may also comprise multiple steps with different ICP powers to control the surface profile of the anti-reflective surface pattern.
- the patterned resist layer may be formed from one of: A1 2 0 3 particles; Au particles; Si0 2 particles; evaporated Au; and FOx e-beam resist.
- the resist is selected to be tolerant to a controlled deep etch.
- a resist may be selected to be compatible with the formation of surface etch features having a height equal to or greater than 2 ⁇ , 4 ⁇ , 6 ⁇ , 8 ⁇ , or 10 ⁇ .
- Cyclic etching using different etch chemistries may also be utilized to control the etching and patterning process.
- halogen based etches such as chlorine-argon plasma etches may also be used in addition to, for example, oxygen plasma etching as described above.
- Such an interference lithography technique for patterning the resist may be combined with a low surface/sub-surface crystal damage etching technology as a route to providing a commercially viable way of fabricating diamond optical windows with low absorbance, low reflectance, and a high laser induced damage threshold for high power laser applications.
- Figure 2 shows a schematic illustration of a portion of an anti-reflective pattern in a surface of a synthetic diamond optical element indicating depth, width, and periodicity dimensional parameters.
- the present applicant has found that increasing the periodicity of moth-eye surface structures in diamond materials has a twofold benefit as described below.
- the first benefit of increasing the periodicity of moth-eye surface structures in diamond materials is that the anti-reflective properties of the diamond surface become less sensitive to deviations from ideal structure geometry that occur within the plane of the surface. This has a significant effect in increasing the margin for error during the moth-eye fabrication process.
- the second benefit of increasing the periodicity the periodicity of moth-eye surface structures in diamond materials is that the aspect ratio of the etched areas can be reduced for an ideal moth-eye surface. This is because the ideal etch depth is constant for any structure periodicity and because the ideal surface pattern's fill fraction changes only slightly with increased periodicity. Fill fraction is defined as (area of surface structure in one periodic unit)/(area of entire periodic unit).
- the optical surface pattern should have a fill fraction within a defined range, the fill fraction defined as [area of projection in one periodic unit]/[area of the periodic unit].
- This area based 2-dimension fill fraction parameter has been found to be important to functional performance and is distinct from a 1 -dimensional fill factor parameter defined as [width of projection]/[length of periodic unit].
- the lithographic processing of diamond doesn't result in perfectly shaped projections and thus a 1 -dimensional fill factor parameter cannot be readily converted into a 2-dimensional fill factor parameter.
- an optical element comprising: synthetic diamond material; and an anti-reflective surface pattern formed directly in at least one surface of the synthetic diamond material, wherein the anti-reflective surface pattern comprises a plurality of projections separated by trenches, the projections spaced apart with a periodicity d, wherein the periodicity d is between 65 and 99% of a zeroeth order diffraction limit above which non zeroeth diffraction orders are observed at an operating wavelength ⁇ , wherein the optical surface pattern has a fill fraction in a range 0.1 to 0.6, the fill fraction defined as [area of projection in one periodic unit]/[area of the periodic unit], and wherein the optical element has an absorption coefficient measured at room temperature of ⁇ 0.2 cm "1 at a wavelength of 10.6 ⁇ .
- the periodicity d is the spacing of projections in the anti-reflective surface pattern and can be determined by measuring the distance between the centres of adjacent projections (or more generally the distance from a point on one projection to a corresponding point on an adjacent projection).
- an ideal anti-reflective surface pattern will be one which is perfectly periodic such that the spacing between any two adjacent projections in the anti-reflective surface pattern is identical to any other two adjacent projections in the anti-reflective surface pattern.
- the periodicity d is between 65 and 99% of the zeroeth order diffraction limit, small deviations or variations in the anti-reflective surface pattern can be tolerated.
- An average periodicity over a number of projections can easily be determined by measuring the distance over a number of projections n and then dividing by (n-1). In this case, the average periodicity should be between 65 and 99% of the zeroeth order diffraction limit.
- the periodicity d may be no less than 70%>, 80%>, 85%, or 87% of the zeroeth order diffraction limit and/or no more than 97%, 95%, or 92% of the zeroeth order diffraction limit and/or any combination of these upper and lower limits.
- the operating wavelength ⁇ may be selected from one of: 10.6 ⁇ ; 2.2 ⁇ ; 1.06 ⁇ ; 532 nm; 355 nm; or 266 nm but is not limited to these wavelengths.
- the zeroeth order diffraction limit is 4.45 ⁇
- the periodicity d of the anti-reflective surface pattern is in a range 3 to 4.40 ⁇ .
- the periodicity d may be no less than 3.20 ⁇ , 3.40 ⁇ , 3.60 ⁇ , or 3.80 ⁇ and/or no more than 4.30 ⁇ , 4.20 ⁇ , or 4.10 ⁇ and/or any combination of these upper and lower limits.
- the zeroeth order diffraction limit for the periodicity d above which non zeroeth diffraction orders are observed at an operating wavelength ⁇ may be calculated as follows:
- the trenches of the anti-reflective surface pattern may have a depth-to -width aspect ratio of less than 3, 2, or 1.5.
- Such relatively wide trenches are more readily fabricating into diamond materials in a more precise manner.
- the desired depth of the trenches remains constant at about 1.72 microns as structure periodicity is increased. Reduction in aspect ratio when increasing structure periodicity stems from increasing the width of the area etched. Aspect ratio of trenches is limited to a minimum of about 1.2 due to appearance of non-zero grating orders when further increasing structure periodicity.
- Anti-reflective surface patterns may comprise projections which have a variety of shapes including, for example, squares, rectangles, cylinders, holes, or hexagons. Sidewalls may also have some amount of taper. It has been found that the required aspect ratio of the trenches is also dependent upon the shape of the structures being etched. For example, it has been found that anti-reflective surface patterns comprising projections which have a square or rectangular cross-sectional shape are advantageous compared to cylinders. Periodic square structures maintain a constant separation (and therefore aspect ratio) along each face for a given fill fraction and periodicity. When considering cylindrical structures of the same fill fraction and periodicity, the minimum separation between cylinders will be significantly less than that of the constant separation of square structures.
- FIG. 3 shows a schematic illustration of anti-reflective surface patterns having cylindrical and square projections indicating that anti-reflective surface patterns comprising square projections have a wider etched area and a lower depth-to-width aspect ratio.
- Figure 4 shows a graph illustrating how reflectivity changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising cylindrical projections with a periodicity of 2.12 ⁇ and a depth of 1.72 ⁇ . For this periodicity and depth, at an operating wavelength of 10.6 ⁇ the ideal radius for the cylindrical projections is 0.88 ⁇ as indicated by the lower line in the graph (% reflection is zero at 10.6 ⁇ for this geometry).
- Figure 5 shows a graph illustrating how reflectivity changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising square projections with a periodicity of 2 ⁇ and a depth of 1.72 ⁇ .
- an antireflective surface pattern comprising square projections with a periodicity of 2 ⁇ and a depth of 1.72 ⁇ .
- a similar effect is observed to that illustrated in Figure 4 for cylindrical projections.
- the ideal side length for the square projections is 1.48 ⁇ as indicated by the lower line in the graph (% reflection is zero at 10.6 ⁇ for this geometry).
- Figure 6 shows a graph illustrating how reflectivity changes with a change in surface geometry, as may be caused by deviations from an ideal surface structure due to imperfect processing during fabrication of an optical element, for an antireflective surface pattern comprising square projections with a periodicity of 4 ⁇ and a depth of 1.72 ⁇ .
- this graph illustrates that an increase in periodicity leads to a reduction in the sensitivity of reflectance to variations in surface geometry.
- the ideal side length for the square projections is 2.65 ⁇ as indicated by the lower line in the graph (% reflection is zero at 10.6 ⁇ for this geometry).
- the reflectivity at an operating wavelength of 10.6 ⁇ increases by only a small amount as illustrated by the upper line in the graph (% reflection is still below 1% at 10.6 ⁇ for this geometry).
- the diamond optical element may also have one or more of the following characteristics: an absorption coefficient measured at room temperature of ⁇ 0.5 cm “1 , ⁇ 0.4 cm “1 , ⁇ 0.3 cm “1 , ⁇ 0.2 cm “1 , ⁇ 0.1 cm “1 , ⁇ 0.07 cm “1 or ⁇ 0.05 cm “1 at a wavelength of 10.6 ⁇ ; a reflectance, at the surface comprising the antireflective surface pattern, of no more than 2%, 1.5%, 1%, or 0.5% at an operating wavelength of the optical element; and a laser induced damage threshold meeting one or both of the following characteristics: the laser induced damage threshold is at least 30 Jem “2 , 50 Jem “2 , 75 Jem “2 , 100 Jem “2 , 150 Jem “2 , or 200 Jem “2 measured using a pulsed laser at a wavelength of 10.6 ⁇ with a pulse duration of 100 ns and a pulse repetition frequency in a range 1 to 10 Hz; and the laser induced damage
- Absorbance, reflectance, and laser induced damage threshold of an optical element are readily measurable by those skilled in the art (for example, ISO 21254-2:2011 describes methods for measuring laser induced damage threshold while Sussmann et al. [Diamond and Related Materials, 3, 1173-117, 1994] describe the specific application of laser damage testing to CVD diamond windows).
- the operating wavelength is selected from one of: 10.6 ⁇ ; 1.06 ⁇ ; 532 nm; 355 nm; or 266 nm, with an operating wavelength of 10.6 ⁇ being preferred for certain commercial applications.
- a synthetic diamond optical element which has low absorbance and low reflectance in combination with low surface damage and an increased laser induced damage threshold. This is considered to be a key combination of parameters for high power laser windows and other high power laser optics such as prisms and lenses.
- the diamond optical element may also have one or more of the following characteristics: a transmittance of at least 95%, 97%, 98% or 99% at the operating frequency of the optical element; a total integrated scatter in a forward hemisphere no more than 2%, 1%, 0.5%, or 0.1% at the operating frequency of the optical element; a dielectric loss coefficient tan ⁇ measured at room temperature at 145 GHz of ⁇ 2 x 10 "4 , ⁇ 10 "4 , ⁇ 5 x 10 "5 , ⁇ 10 "5 , ⁇ 5 x 10 “6 , or ⁇ 10 "6 ; an average micro feature density no greater than 5 mm “2 , 3 mm “2 , 1 mm “2 , 0.5 mm “2 , or 0.1 mm “ ; a micro feature distribution such that there are no more than 5, 4, 3, 2, or 1 microfeatures within any 3 mm 2 area; an integrated absorbance per unit thickness of no more than 0.20 cm “2 , 0.15 cm “2 ,
- microfeatures are micron scale features present in polycrystalline CVD diamond material (i.e. bulk material features rather than surface features) and are believed to be the result of microcracks and/or sp2 carbon within the polycrystalline CVD diamond material. These features can be observed, measured, and counted by optical analysis. The upper limits for microfeature density and distribution for a particular application will be dependent on the size of the microfeatures and on the position of the microfeatures in the diamond optical element.
- the average microfeature density may be ⁇ 0.3/mm 2 for microfeatures having a diameter range 50 ⁇ to 150 ⁇ , ⁇ 0.08/mm 2 for microfeatures having a diameter range 150 ⁇ to 350 ⁇ , and 0 microfeatures/mm 2 for microfeatures with a diameter > 350 ⁇ .
- the microfeature distribution may be such that for microfeatures having a diameter range 50 ⁇ to 150 ⁇ there are no more than 150 microfeatures within a 20 mm diameter of the optical component and no more than 350 microfeatures within a 20 to 40 mm diameter of the optical component.
- microfeatures having a diameter range 150 ⁇ to 350 ⁇ there may be no more than 25 microfeatures within a 20 mm diameter of the optical component and no more than 100 microfeatures within a 20 to 40 mm diameter of the optical component.
- microfeatures having a diameter greater than 350 ⁇ there may be no microfeatures anywhere in the optical component.
- Such optical characteristics can be achieved by applying the patterning technology as described herein to high quality optical grades of synthetic diamond material, such as high quality optical grade polycrystalline CVD diamond available from Element Six Limited. It is also envisaged that the patterning technology may be applied to optical grade single crystal CVD diamond (also available from Element Six Limited) for certain optical applications. Furthermore, in addition to polycrystalline diamond material and single crystal diamond material, the patterning technique as described herein may also be applied to tiled single crystal diamond plates in which a plurality of single crystal diamond substrates are inter- grown to form a single optical plate comprising a plurality of single crystal diamond windows or an effectively single crystal large area diamond plate. The patterning technique may also be applied to hetero-epitaxially grown single crystal diamond material.
- the optical element meets one or more of the optical characteristics as described herein over at least 50%, 60%, 70%, 80%, 90%, or 100% of the area of the surface of the diamond optical element on which the anti-reflective diffractive surface finish is formed.
- diamond optical elements can be fabricated to relatively large areas.
- synthetic diamond components can be fabricated to a have largest linear dimension of at least 5 mm, 10 mm, 20 mm, 40 mm, 60 mm, 80 mm, 100 mm, 120 mm, or 140 mm.
- Such synthetic diamond components may be fabricated with a thickness equal to or greater than 200 ⁇ , 250 ⁇ , 350 ⁇ , 450 ⁇ , 500 ⁇ , 750 ⁇ , 1000 ⁇ , 1500 ⁇ , or 2000 ⁇ .
- the synthetic diamond material is fabricated by growing to a target thickness greater than that required for the final optical element and then processing a nucleation face of the diamond material to remove early stage nucleation diamond.
- a target thickness greater than that required for the final optical element leading to a reduction in thermal conductance and an increase in optical absorbance.
- By growing the synthetic diamond material to a target thickness greater than that required for the final optical element it is possible to remove early stage nucleation diamond and thus provide an optical element with higher thermal conductance and lower optical absorbance. Removal of early stage nucleation diamond will inevitably result in a slight reduction in the strength of the synthetic diamond material.
- manufacturers such as Element Six Limited are capable of fabricating thick wafers of synthetic diamond material, such as polycrystalline CVD diamond wafers, with a high tensile rupture strength which enables removal of early stage nucleation diamond while retaining sufficient mechanical strength for end applications.
- the synthetic diamond material may have one or more of the following structural characteristics: a tensile rupture strength with a nucleation face of the synthetic diamond material in tension of: > 760 MPa x n for a thickness of 200 to 500 ⁇ ; > 700 MPa x n for a thickness of 500 to 750 ⁇ ; > 650 MPa x n for a thickness of 750 to 1000 ⁇ ; > 600 MPa x n for a thickness of 1000 to 1250 ⁇ ; > 550 MPa x n for a thickness of 1250 to 1500 ⁇ ; > 500 MPa x n for a thickness of 1500 to 1750 ⁇ ; > 450 MPa x n for a thickness of 1750 to 2000 ⁇ ; or > 400 MPa x n for a thickness of > 2000 ⁇ , wherein multiplying factor n is 1.0, 1.1, 1.2, 1.4, 1.6, 1.8, or 2; and a tensile rupture strength with a growth face of the synthetic diamond material in tension of: >
- Such synthetic diamond material may be processed to a surface flatness ⁇ 5 ⁇ , ⁇ 4 ⁇ , ⁇ 3 ⁇ , ⁇ 2 ⁇ , ⁇ 1 ⁇ , ⁇ 0.5 ⁇ , ⁇ 0.2 ⁇ , ⁇ or 0.1 ⁇ and/or a surface roughness R a no more than 200 nm, 150 nm, 100 nm, 80 nm, 60 nm, 40 nm, 20 nm, or 10 nm.
- the R a limit is in part determined by operating wavelength. The aforementioned limits apply for mid and far IR operating wavelengths. For visible operating wavelengths, the R a limit will typically be lower. In this regard, it will be noted that for single crystal diamond materials an R a much lower than 10 nm is achievable.
- the synthetic diamond material may comprise at least a portion which has a 13 C content of less than 1.0%, 0.8%, 0.6%, 0.4%, 0.2%, 0.1%, 0.05%, or 0.01%.
- isotopically purified carbon source gas is expensive.
- one or more surface layers of the synthetic diamond material may be formed of isotopically purified diamond material with the interior bulk being fabricated using a higher 13 C content, preferable natural abundance.
- a surface layer comprising the anti-reflective surface pattern is formed of isotopically purified diamond material so as to increase the thermal conductivity of the anti-reflective surface pattern and thus reduce localized heating and increase the laser induced damage threshold of the anti- reflective surface pattern.
- An underlying portion of synthetic diamond material may then comprise a higher concentration of 13 C, preferably natural abundance, to reduce synthesis costs.
- the anti-reflective surface finish of the present invention may be formed over the majority of a surface of the synthetic diamond material, e.g. over at least 50%, 60%, 70%>, 80%>, 90%>, or over the entire surface.
- the anti-reflective diffractive surface finish can be formed over an area of at least 25 mm 2 , 50 mm 2 , 100 mm 2 , 200 mm 2 , 300 mm 2 , 500 mm 2 , 700 mm 2 , 1000 mm 2 , 1500 mm 2 , 2000 mm 2 , 3000 mm 2 , 5000 mm 2 , 7000 mm 2 , 10000 mm 2 , 15000 mm 2 , or 20000 mm 2.
- the surface which is patterned with the anti-reflective surface finish may, for example, form the major optical exit and/or entry face of a diamond window, lens or prism with a majority, or the entire, optical exit and/or entry face of the optical element being patterned with an anti- reflective diffractive surface finish. In some applications it may be desirable to leave an unpatterned portion around a peripheral region of the transmissive optical element for mounting the transmissive optical element.
- the anti-reflective surface pattern is formed on at least two surfaces of the synthetic diamond material.
- the anti- reflective diffractive surface finish can be formed on both the optical entry face and the optical exit face of the optical element, e.g. on opposing major faces of a diamond window.
- low reflectance is only required on one surface of the optical element, e.g. a beam splitter where partial reflectance is required on one surface.
- the present invention has been described above in the context of providing a synthetic diamond optical element comprising an anti-reflective surface pattern formed directly in the surface of synthetic diamond material.
- a synthetic diamond optical element comprising a birefringent surface pattern formed directly in the surface of the synthetic diamond material and which has low surface and subsurface crystal damage thus exhibiting a high laser induced damage threshold.
- Such birefringent surface patterns can be formed directly in the surface of synthetic diamond material using the fabrication techniques as described herein.
- an antireflective surface pattern and a birefringent surface pattern comprises elongate projections which are used for manipulation of polarization. That said, while their end uses can be quite different, antireflective surface patterns and birefringent surface patterns as described herein follow the same design guidelines in terms of periodicity. It may also be noted that birefringent gratings will also reduce reflections at the surface in which they are disposed, but the reflections will not be reduced to the degree they would be for an optimized antireflective surface pattern. For example, reflection at a birefringent surface pattern will be around 7 or 8% depending on the exact design of the birefringent pattern. Thus, according to certain configurations, an optical element may be provided with a birefringent surface pattern formed in one surface of the synthetic diamond material and an antireflective surface pattern formed in an another surface of the synthetic diamond material.
- Birefringent subwavelength gratings can be formed in the surface of synthetic diamond with the necessary etch depth to create either a quarter or half waveplate.
- This approach has a number of advantages over traditional waveplates.
- synthetic diamond possesses a very high laser induced damage threshold and is an excellent conductor of heat at room temperatures. This means that a waveplate grating fabricated in diamond can be used in the most demanding high power laser applications without being damaged and without suffering detrimental thermal effects typical of other materials.
- birefringent subwavelength grating To make a birefringent subwavelength grating simply requires features with asymmetric dimensions along the x and y axes.
- the simplest design for a birefringent subwavelength grating is a linear grating where the periodicity of the lines is below the subwavelength limit.
- other simple designs include structures that are rectangular (but not square) or elliptical. These structures can be etched into the surface of diamond using processing techniques as described herein.
- the grating When light interacts with a subwavelength grating the grating is treated as though it were a uniform material with a certain refractive index.
- the grating can essentially be considered a thin film with an effective refractive index between that of the incident medium and that of the substrate.
- the effective index of the grating When the subwavelength grating structures are asymmetric between the x and y axes, the effective index of the grating also becomes asymmetric between the x and y axes.
- the asymmetric grating is treated as a birefringent medium with a "fast" and a "slow" axis.
- the depth of the birefringent subwavelength grating it is possible to design a grating with a set amount of retardance between polarization states along the fast vs slow axes.
- the retardance By designing the retardance to be either a quarter or half wave makes the grating an effective quarter or half waveplate.
- FIG. 7 shows a schematic illustration in plan view of a portion of a birefringent pattern in a surface of a synthetic diamond optical element, the birefringent pattern comprising an elongate projection with elongate trenches disposed either side of the elongate projection.
- Figure 8 shows a schematic illustration in cross-sectional view of a birefringent surface pattern having elongate projections which has a trapezoidal cross-sectional shape.
- Optimization is performed by using a 2D parameter sweep over etch depth and linewidth while recording data for amount of retardation and grating transmission.
- the parameters that give the desired amounts of retardation are then selected out and plotted in terms of transmission.
- Our optical modelling software has been shown to accurately predict real world results in terms of both transmission and retardance.
- Figure 9 shows transmission vs linewidth and etch depth for parameters that result in either half wave or quarter wave retardance.
- Optimal design is determined by balance between high transmission and manufacturability. This optimization assumes periodicity of 4 ⁇ , a sidewall taper of 5°, and a design wavelength of 10.6 ⁇ .
- Advantages of a birefringent subwavelength grating in diamond over a traditional waveplate include: greater laser induced damage threshold; higher thermal conductivity material; size limited only by available size of diamond windows; and provision of a true zero-order waveplate.
- Optical elements fabricated from high quality optical grade synthetic diamond material and comprising an optical surface pattern as described herein are suitable for use in high power optical systems due to their low reflectance and high laser induced damage threshold.
- an optical system as illustrated in Figure 10 comprising: a synthetic diamond optical element 10 comprising an optical surface pattern as described herein; and a light source 12 (e.g. a laser) configured to generate light 14 at a power of at least 300W, 500W, 1 kW, 3 kW, 5 kW, 10 kW, 15 kW, 20 kW, 25 kW, 30 kW, 35 kW, 40 kW, 45 kW, or 50 kW and transmit said light through the synthetic diamond optical element 10.
- a light source 12 e.g. a laser
- the operating power of the described optical system is significantly lower that the previously defined continuous wave laser induced damage threshold of 1 MW/cm 2 .
- the laser induced damage threshold of the synthetic diamond optical element should be significantly higher than the operating power of the optical system.
- Laser induced damage threshold is one of the key motivations for embodiments of this invention and is measured in terms of power density.
- high power density does not necessarily mean high operating power although high operating power typically goes with high power density.
- Current systems are now operating at a power density between 1 and 10 kW/cm 2 with further increases towards 100 kW/cm 2 anticipated.
- the light source 12 e.g.
- a laser may thus be configured to generate light 14 at a power density of at least 1 kW/cm 2 , 3 kW/cm 2 , 5 kW/cm 2 , 10 kW/cm 2 , 20 kW/cm 2 , or 50 kW/cm 2 , and transmit said light through the synthetic diamond optical element 10.
- the optical element 10 is in the form of a transmissive diamond window with an optical surface pattern 16 fabricated in both major faces of the window.
- the optical system may also provide a cooling system for cooling the synthetic diamond optical element.
- the present inventors have noted that Element Six's optical grade synthetic diamond material shows a large decrease in absorption at low temperatures. This effect is not seen to the same extent with certain other diamond materials.
- optical elements as described herein comprise the key combination of parameters for high power laser windows.
- embodiments of the present invention are considered to be an enabling technology for high power laser systems.
- optical elements as described herein may be used in broad band visible wavelength applications (e.g. watch faces) where anti-reflective surface finishes may be provided for their mechanical robustness relative to thin film coatings.
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Abstract
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EP15727675.9A EP3155460B1 (en) | 2014-06-16 | 2015-06-10 | Synthetic diamond optical elements |
JP2016573538A JP2017521699A (en) | 2014-06-16 | 2015-06-10 | Synthetic diamond optical element |
US15/316,799 US10809420B2 (en) | 2014-06-16 | 2015-06-10 | Synthetic diamond optical elements |
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GBGB1417982.4A GB201417982D0 (en) | 2014-10-10 | 2014-10-10 | Synthetic diamond optical elements |
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GB2527422A9 (en) | 2017-05-17 |
EP3155460B1 (en) | 2023-01-04 |
JP2019070837A (en) | 2019-05-09 |
JP2021096484A (en) | 2021-06-24 |
EP3155460A1 (en) | 2017-04-19 |
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JP2017521699A (en) | 2017-08-03 |
GB201510100D0 (en) | 2015-07-22 |
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US20170242158A1 (en) | 2017-08-24 |
US10809420B2 (en) | 2020-10-20 |
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